Prepn process of nanometer granular Fe3O4

A particle and nano technology, applied in the nano field, can solve the problems of poor dispersion effect and high cost of centrifugal separation

Inactive Publication Date: 2003-06-04
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses centrifugation to prepare ferroferric oxide nanoparticles at a high cost. From the published results, it can be seen that the final dispersion effect is not good. When coating, more single ferric oxide nanoparticles are coated together. The phenomenon

Method used

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  • Prepn process of nanometer granular Fe3O4

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Embodiment 1

[0013] Under the protection of N2, slowly add 1.0mol / l ammonia solution to 2.0mol / l FeCl at 30°C 3 and 1.0mol / lFeCl 2 Mix the solution in 300ml until PH=12. Continue stirring for a quarter of an hour. Then filter and wash. Put 2 grams of nanoparticles of iron ferric oxide prepared in 200 ml of distilled water, adjust the pH to 1 with HCl, add 1.2 grams of sodium dodecylbenzenesulfonate, and react for 2 hours under the action of ultrasonic waves and stirring, and the temperature is controlled Between 10°C and 40°C. The modified iron ferric oxide nanoparticles are filtered and washed, and dispersed in the organic solvent toluene.

Embodiment 2

[0015] Under the protection of N2, slowly add 0.5mol / l ammonia solution to 4.0mol / l FeCl at 50°C 3 , 3.0mol / lFeCl 2 and 0.001mol / l CrCl 3 Mix the solution in 250ml until PH=12. Continue stirring for a quarter of an hour. Then filter and wash. Put 1 gram of ferric oxide nanoparticles in distilled water at 100°C, adjust the pH to 2 with HCl, add 1.2 grams of sodium dodecylbenzenesulfonate, and react for 3 hours under the action of ultrasonic waves and stirring. Between 10°C and 40°C. The modified iron ferric oxide nanoparticles are filtered and washed, and dispersed in the organic solvent toluene.

Embodiment 3

[0017] Under the protection of N2, slowly add 1.5mol / l ammonia solution to 5.0mol / l FeCl at 90°C 3 and 4.0mol / lFeCl 2 Mix the solution in 300ml until PH=12. Continue stirring for a quarter of an hour. Then filter and wash. Put 5 grams of ferric oxide nanoparticles prepared in 150ml of distilled water, adjust the pH to 3 with HCl, add 1.0 grams of sodium oleate, and react for 2 hours under the action of ultrasonic waves and stirring, with the temperature controlled at 10°C-40°C between ℃. The modified iron ferric oxide nanoparticles are filtered and washed, and dispersed into the organic solvent styrene.

[0018] The invention is in N 2 To protect the environment, gradually add 0.5-1.5mol / l ammonia water to FeCl at 30°C-50°C 3 and FeCl 2 In the mixed solution of FeCl 3 and FeCl 2 The molar ratio of the two is: 4:3-2:1, and react for 1-2 hours under high-speed stirring. The formed Fe3O4 particles were separated and the excess particles were washed off with distilled wa...

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Abstract

The preparation process of nano granular Fe3O4 includes the steps of: dropping ammonia water to mixed FeCl3 and FeCl2 solution in protective N2 environment for reaction while high speed stirring; separating Fe3O4 grains and washing with distilled water to eliminate excessive grains, setting the washed Fe3O4 grains into distilled water, adding acid to regulate pH to 1-4, adding anionic surfactant in 0.2-4 % to react under ultrasonic stirring, separating and washing Fe3O4 grains and setting Fe3O4 grains in organic solvent. During the process metal ion may be added in the first step and the anionic surfactant is sodium oleate, sodium dodecyl benzene sulfonate, etc. The prepared Fe3O4 grains have good dispersivity and low cost.

Description

technical field [0001] The invention belongs to nanotechnology, in particular to a method for preparing nano-Fe 3 o 4 particle method. Background technique [0002] Nano-ferrite particles have aroused great interest because of their important application value in magnetic fluid and magnetic recording. Especially, nano-ferrite particles encapsulated by polymers have great application value in medical detection. How to prepare monodisperse nano-ferrite particles with superparamagnetism is an important research field in chemistry and material science. There have been many reports about monodisperse ferric oxide ultrafine particles at home and abroad, but the nanoparticles obtained by common chemical methods have poor monodispersity and are easy to agglomerate. [0003] Lei Fu et al. published their work in Applied Surface Science (No. 181, 2001, P173-178). They used the co-precipitation method to prepare ferric oxide nanoparticles, and coated the surface with lauric acid an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 刘祖黎姚凯伦刘永基陶晋丁宗华王欣龚非力
Owner HUAZHONG UNIV OF SCI & TECH
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